The Journey Begins Design of Experiment and APT ...€¦ · LEAP raw data. With FeCr . density...
Transcript of The Journey Begins Design of Experiment and APT ...€¦ · LEAP raw data. With FeCr . density...
The Journey BeginsDesign of Experiment and APT
Preparation for Success1ST PRE-MEETING CONGRESS ON ATOM PROBE TOMOGRAPHY (APT)
Richard L. MartensCentral Analytical Facility
The University of Alabama
M&M 2016 JULY 24TH
Alternate Titles• DOE&APT, Yup. You Know Me• Trial by Fire• DAMN My Ambition• What the Hell was I Thinking?
https://www.isixsigma.com/tools-templates/design-of-experiments-doe/design-experiments-%E2%90%93-primer/
Design of experiments (DOE) is a systematic method to determine the relationship between factors affecting a process and the output of that process. In other words, it is used to find cause-and-effect relationships. This information is needed to manage process inputs in order to optimize the output
Material (Sample)
Specimen Preparation &
Instrument Parameters
Data/No Data
Microstructure & Environment
Better Check Yourself
• “Who” is my material? – Evaporation fields– Mechanical Properties?
• What are the questions? – Composition? Microstructure? Clustering?
• WHEN? How much time do I plan to invest?• WHERE is my ROI?• Why APT?
UA-CAF Research Instrumentation
FEI Quanta 200 3D Dual-beam
FIB
JEOL 7000 FEG SEMOxford Aztec EDS,
EBSD, WDS E-beam litho
Chemical mapping
EBSD camera
Electron probe
2 theta
(110)(100)
Specimen
(111)OIM
Site-specific sample prep
Bruker GADDS XRD
FEI TECNAI F20 TEM
2 nm2 nm
High-res imaging
Local Electrode Atom Probe
atom map
Rapid phase ID
Chemical bonding
1-, 2- and 3-D characterization capability from the atomic scale to hundreds of microns – >106
orders of magnitude in imaging capability!
KRATOS AXIS 165 XPS
TESCAN LYRA XMU FIB-FESEM
atom probe preparation
TEM preparation
Qualitative phase ID
Precession Electron Diffraction of Atom Probe Specimens
JEOL 8600 EPMA
WDS –Qualitative Analysis
CAMECA LEAP 5000
EDAX TEAM EBSD, EDS
Bruker EDS & GATAN CL
Four Main Components of an APT Specimen
SAMPLESPECIMEN
“Wedge” or “Lift-Out”
PLATINUM (Pt-weld, Pt-dep) SHARPENING
(Tip Radius/Geometry)
Environmental Factors:Specimen Preparation
• Ion beam damage and “re-deposition”• Quality of platinum weld• Tip shape/geometry
– Apex– Post
• DOCUMENT!!! Record images• Be careful about e-beam contamination
Platinum Deposition (Weld, Brazing)
Sharpening
Edges or No Edges?
Document!
Measure & Record!
The GOOD
The BAD
The UGLY
Show Me the Data
Specimen “Yield” Rate
LEAP Instrument Parameters
• Laser vs. Voltage mode• Temperature• Pulse Rate• Pulse Fraction• Laser Energy
Less Stress, More Resolution, Please
“Improving Data Quality in APT” D.J. Larson, et al, M&M 2014 proc
Specimen vs. Electrode
POST MORTEM ANALYSIS
50 nm
100 nm
100 nm
PED Orientation Image
TEMLEAP raw data
With FeCr density isosurface
TEM BF image before
PED scanning
TEM BF image after
PED scanning
Correlative Analysis
Xuyang ZhouUA-Graduate student
Greg Thompson Group
CORRELATE & COLLABORATE
“Influence of Fe(Cr) miscibility on thin film grain size and stress” Xuynag Zhou, et al, Thin Solid Films 2016
FOLLOW THE SOP’s
• “Specimens will either run or not run”– Mike Miller
• “When specimens work, it is good. When they do not work, things are very difficult”– Kazuhiro Hono
Summary